CN1053412A - The bicarbonate of ammonia neutralisation is produced zinc oxide - Google Patents
The bicarbonate of ammonia neutralisation is produced zinc oxide Download PDFInfo
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- CN1053412A CN1053412A CN 90100299 CN90100299A CN1053412A CN 1053412 A CN1053412 A CN 1053412A CN 90100299 CN90100299 CN 90100299 CN 90100299 A CN90100299 A CN 90100299A CN 1053412 A CN1053412 A CN 1053412A
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- zinc oxide
- bicarbonate
- ammonia
- zinc
- neutralisation
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Abstract
The present invention relates to a kind of bicarbonate of ammonia (NH that utilizes
4HCO
3) neutralisation is produced the method for zinc oxide (ZnO), is the important reform that utilizes the soda ash neutralisation to produce zinc oxide (ZnO) to existing.Because the present invention adopts bicarbonate of ammonia (NH
3HCO
3) replacement price soda ash (Na higher and in short supply
2CO
3) carry out neutralization reaction and make zinc oxide (ZnO), this has just reduced the cost of zinc oxide, and can obtain having the byproduct chemical fertilizer ammonium sulfate of important economic worth.
Description
The present invention relates to a kind of preparation method of oxide compound, is a kind of method of utilizing the bicarbonate of ammonia neutralisation to produce zinc oxide specifically.
The existing method of producing zinc oxide, adopt the zinc carbonate decomposition methods produce zinc oxide (according to Tianjin Chemical Engineering Inst., Ministry of Chemical Industry " the 552nd page of Chemicals handbook nineteen eighty-two version), with zinc gray, sulfuric acid, soda ash is main raw material, with dilute sulphuric acid with metallic zinc and compound dissolution thereof in the zinc gray after, make solution of zinc sulfate, after removing impurities by oxidation matter, add soda ash solution again, carry out neutralization reaction, synthetic zinc subcarbonate, see that shown in the accompanying drawing 1, its reaction equation is as follows:
Through washing, solid-liquid separation, again with the oven dry of zinc subcarbonate filter cake, calcining, the pulverizing that make, just make the zinc oxide finished product, see shown in the accompanying drawing 1 that this technology is because the higher soda ash in short supply of use value is raw material, so cost is higher, and contain a large amount of saltcake in the waste water after production process, easy contaminate environment.
Adopt the present invention to produce zinc oxide and use bicarbonate of ammonia without soda ash instead, other main raw material (zinc gray, sulfuric acid etc.) and the norm quota of consumption thereof are same as the prior art, so just, greatly reduce cost, when producing zinc oxide with the present invention, can obtain important economic worth chemical fertilizer ammonium sulfate, and eliminate the contaminated wastewater after prior art is produced zinc oxide.
The present invention is achieved in that existing and manufactures in the technical process of zinc oxide, replaces soda ash with bicarbonate of ammonia, carries out neutralization reaction with zinc sulfate, generates zinc subcarbonate, is made through washing, drying, pulverizing and calcining again.
Accompanying drawing 1 is produced the zinc oxide process flow sheet for the soda ash neutralisation.
Accompanying drawing 2 is produced the zinc oxide process flow sheet for the bicarbonate of ammonia neutralisation.
Below in conjunction with accompanying drawing 2 technological process of production of the present invention is done detailed argumentation.
(1) complex acid: in the acid proof enamel jar, add gauge water, under agitation slowly add the vitriol oil, be made into the dilute sulphuric acid of 20 Baumes, when temperature surpasses 90 ℃, lower the temperature indirectly with cold water.
(2) change zinc: to dilute sulphuric acid (H
2SO
4) in add zinc gray (ZnO) slowly, do not stop to stir, when the solution pH value is raised to PH
4The time, stop to feed in raw material.Reaction equation is:
(3) reduction: under constantly stirring to zinc sulfate (ZnSO
4) add a spot of zinc powder (decide), adding at twice in the solution according to copper Cu, nickel, cadmium Cd content in the zinc gray.Inspection by sampling, filtrate must reach water white transparency, filters with flame filter press then, and filtrate is sent into the once oxidation jar with impeller pump.Reaction equation is as follows:
(4) once oxidation: under constantly stirring, the caustic soda of careful adding a spot of 18% is transferred to PH with the pH value of filtrate in zinc sulfate filtrate
5, slowly add potassium permanganate (KMnO again
4) solution (5%), make potassium permanganate (KMnO
4) excessive slightly, solution shows potassium permanganate (KMnO
4) characteristic color (lavender).Keep 80-90 ℃ of temperature, stirred 1 hour.Filter, filtrate is sent into the secondary oxidation jar with impeller pump.Reaction equation
(5) secondary oxidation: after the lavender of filtrate fades away, in filtrate, add a small amount of potassium permanganate (KMnO again
4), constantly stir, holding temperature 80-90 ℃, oxidation 1 hour.Sample thief filters with potassiumiodide-starch solution after the assay was approved, and filtrate is sent into neutralization tank with impeller pump.Reaction equation is with an oxidation equation formula.
(6) neutralization; The 9 Baume bicarbonate of ammonia (NH that make earlier will be given
4HCO
3) solution slowly joins in the neutralization tank.Ceaselessly stir, stirring velocity is at 15-25 rev/min, and optimum velocity is at 17 rev/mins, and holding temperature 10-34 ℃, optimum temps maintains 15-25 ℃.In and the time be controlled at about 1 hour, the sampling reach between the PH6.0-7.0 with acidity instrumentation solution PH value, best pH value is controlled at PH6.5-6.8, stops to add bicarbonate of ammonia, restir 30 minutes, stop the stirring.Bicarbonate of ammonia (NH
4HCO
3) and zinc sulfate (ZnSO
4) carry out neutralization reaction, generate zinc subcarbonate, carbonic acid gas and ammonium sulfate, reaction equation is as follows:
(7) washing: above-mentioned thin pulp is clarified half an hour, siphon away upper clear supernate, in order to the reclaim(ed) sulfuric acid ammonium.Add peace and quiet tap water again, stirred 5 minutes, clarify half an hour again, siphon away upper clear supernate, can make liquid fertilizer and use.Till being up to the standards with barium chloride solution with this method rinsing to solution.Filter with flame filter press then, filtrate discards.
(8) drying: filter cake is put into drying baker dry.
(9) pulverize: dried filter cake is ground into meal with pulverizer.
(10) calcining: above meal is sent in the calcining furnace, under 800-900 ℃ of temperature, calcined 2.5 hours, can get qualified product, cooling packing gets product then.Reaction equation is as follows:
The zinc oxide that makes with the present invention has reached the first grade standard of standard GB 3185-82 fully, and zinc oxide content can reach more than 99.7%, and yield reaches 97%, can obtain having simultaneously the byproduct of ammonium sulfate of important economic worth.
Embodiment 1: be made into dilute sulphuric acid with 750 premium on currency and 130 liter of 98% vitriol oil, change zinc gray (containing ZnO84%) 240 kilograms.With 3 kilograms of zinc powder reductions.Use 40 liters of oxidations of 5% potassium permanganate solution (once oxidation) after the filtration again.Use 2 liters of oxidations of 5% potassium permanganate solution (secondary oxidation) after the filtration again.Filter rear filtrate and be diluted with water to 18 Baumes.Use 2880 liters of neutralizations of ammonium bicarbonate soln of 9 Baumes then, neutral temperature is controlled at 10 ℃, in and the terminal point pH value be PH6.0, stirring velocity is 15 rev/mins.Through the rinsing after-filtration.Filter cake is pulverized after the drying in drying baker.Powder is delivered to calcining furnace,, take out cooling then 800-900 ℃ of temperature lower calcination 2.5 hours.Meet standard GB 1385-82 first grade standard fully through the chemical examination quality product, content reaches 99.9%.Real 163.7 kilograms of zinc oxide products, the yield 81.2% of getting.
Embodiment two, are made into dilute sulphuric acid with 1500 premium on currency and 270 liter of 98% vitriol oil, change zinc gray (containing ZnO84%) 500 kilograms.Use 6 kilograms of zinc powder reductions again.Use 80 liters of oxidations of potassium permanganate solution (once oxidation) of 5% after the filtration again.Use 4 liters of oxidations of 5% potassium permanganate solution (secondary oxidation) after the filtration again.Be diluted with water to 18 Baumes after the filtration.Use 5700 liters of neutralizations of ammonium bicarbonate soln of 9 Baumes then.Neutral temperature is controlled at 15-25 ℃, in and the terminal point pH value be PH6.5-6.8, stirring velocity is 17 rev/mins.Through the rinsing after-filtration.Filter cake is pulverized after drying in drying baker.Powder is sent into calcining furnace, 800-900 ℃ of temperature lower calcination 2.5 hours.Take out cooling then.Meet standard GB 1385-82 primary standard, content 99.8% fully through the chemical examination quality product.Real 411 kilograms in zinc oxide, the yield 98% of getting.
Embodiment three, are made into dilute sulphuric acid with 1000 premium on currency and 180 liter of 98% vitriol oil, change zinc gray (containing ZnO49.8%) 560 kilograms.Use 5 kilograms of zinc powder reductions again.Use 60 liters of oxidations of 5% potassium permanganate solution (once oxidation) after the filtration again.Use 3 liters of oxidations of 5% potassium permanganate solution (secondary oxidation) after the filtration again.Be diluted with water to 18 Baumes after the filtration.Use 4090 liters of neutralizations of ammonium bicarbonate soln of 9 Baumes then.Neutral temperature is controlled at 34 ℃, in and the terminal point pH value be PH7.0, stirring velocity is 25 rev/mins.Through the rinsing after-filtration.Filter cake is pulverized after drying in drying baker.Powder is sent into calcining furnace, 800-900 ℃ of temperature lower calcination 2.5 hours.Take out cooling then.Meet standard GB 1385-82 first grade standard, content 99.7% fully through the chemical examination quality product.Real 266.3 kilograms of zinc oxide products, the yield 95.5% of getting.
The present invention greatly reduces the cost of producing zinc oxide, and does not pollute the environment, and can also obtain having the byproduct of ammonium sulfate of important economic worth, has remarkable economic efficiency and social benefit.
Claims (3)
1, a kind of method of utilizing the bicarbonate of ammonia neutralisation to produce zinc oxide, it mainly contains complex acid, changes technological processs such as zinc, reduction, once oxidation, secondary oxidation, neutralization, washing, drying, pulverizing and burning, it is characterized in that: in N-process, adopt bicarbonate of ammonia and zinc sulfate to carry out neutralization reaction, neutral temperature is grasped between 10-34 ℃, in and the terminal point pH value grasp between PH6.0-7.0.
2, the method for utilizing the bicarbonate of ammonia neutralisation to produce zinc oxide according to claim 1, it is characterized in that in and optimum temps be controlled at 15-25 ℃, in and the best pH value of terminal point grasp at PH6.5-6.8
3, describedly produce the method for zinc oxide with the bicarbonate of ammonia neutralisation according to claim 1,2, it is characterized in that in the N-process otherwise stop stirring, stirring velocity is controlled at 15 and goes to 25 rev/mins, and optimum control is at 17 rev/mins.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90100299 CN1053412A (en) | 1990-01-19 | 1990-01-19 | The bicarbonate of ammonia neutralisation is produced zinc oxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90100299 CN1053412A (en) | 1990-01-19 | 1990-01-19 | The bicarbonate of ammonia neutralisation is produced zinc oxide |
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| CN1053412A true CN1053412A (en) | 1991-07-31 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035870C (en) * | 1994-08-11 | 1997-09-17 | 重庆化肥矿山工业公司 | Process for producing high-dispersivity active zinc oxide |
| CN1091748C (en) * | 1998-09-02 | 2002-10-02 | 中国科学院化工冶金研究所 | Powdered nm-class zinc oxide particles cladded by metallic compound on surface and preparation method |
| CN105366706A (en) * | 2014-08-25 | 2016-03-02 | 蒋小华 | Preparation method of nano-sized basic zinc carbonate |
| CN111825125A (en) * | 2020-09-16 | 2020-10-27 | 金驰能源材料有限公司 | Doped basic cobalt carbonate/cobalt carbonate composite precursor and preparation method and application thereof |
| CN112504909A (en) * | 2020-11-07 | 2021-03-16 | 韶关凯鸿纳米材料有限公司 | Method for measuring ammonium bicarbonate content and zinc oxide production process for controlling ammonium bicarbonate dosage |
-
1990
- 1990-01-19 CN CN 90100299 patent/CN1053412A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035870C (en) * | 1994-08-11 | 1997-09-17 | 重庆化肥矿山工业公司 | Process for producing high-dispersivity active zinc oxide |
| CN1091748C (en) * | 1998-09-02 | 2002-10-02 | 中国科学院化工冶金研究所 | Powdered nm-class zinc oxide particles cladded by metallic compound on surface and preparation method |
| CN105366706A (en) * | 2014-08-25 | 2016-03-02 | 蒋小华 | Preparation method of nano-sized basic zinc carbonate |
| CN111825125A (en) * | 2020-09-16 | 2020-10-27 | 金驰能源材料有限公司 | Doped basic cobalt carbonate/cobalt carbonate composite precursor and preparation method and application thereof |
| CN112504909A (en) * | 2020-11-07 | 2021-03-16 | 韶关凯鸿纳米材料有限公司 | Method for measuring ammonium bicarbonate content and zinc oxide production process for controlling ammonium bicarbonate dosage |
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